Hydrochloric Acid → HCID 11165454、化合物

HRID 1963804ノート

反応式

HRID 1963804 の反応式
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([NH2:11])=[N:3]1.[CH2:12]([N:14]([CH2:17][CH3:18])[CH2:15][CH3:16])[CH3:13].[OH-].[Na+].[ClH:21].[CH2:22]([OH:24])[CH3:23]>C1(C)C=CC=CC=1.ClCCl>[ClH:21].[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([NH:11][C:22]([CH:23]2[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][C:5]3[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=3)[CH2:12][CH2:13]2)=[O:24])=[N:3]1

参加物

8

反応物 5

HCID 313Hydrochloric Acid2 回HCID 702Ethanol3 回HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 122913171-Methyl-1H-indazol-3-amine

生成物 1

HCID 11165454HCID 11165454、化合物

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒

実験手順

The product of Example 5b) (1.68 g; 0.006 mol) was added to a solution of 1-methyl-1H-3-indazoleamine (0.86 g; 0.006 mol), prepared as described in the Journal of Heterocyclic Chemistry 1979 (16), 783-784, and of triethylamine (2.4 ml; 0.018 mol) in toluene (20 ml). The reaction mixture was stirred at room temperature for 18 h and then the solvent was removed by evaporation at reduced pressure. The residue thus obtained was taken up with 1N NaOH and dichloromethane and transferred to a separatory funnel. The organic phase was separated, dried over Na2SO4 and the solvent was removed by evaporation at reduced pressure. The product thus obtained was transformed into the corresponding hydrochloride by dissolution in ethanol, addition of hydrogen chloride in ethanol and recrystallization from ethanol, to give the desired salt (1.6 g).

後処理

  1. customprepared
  2. customthe solvent was removed by evaporation at reduced pressure
  3. customThe residue thus obtained
  4. customtransferred to a separatory funnel
  5. customThe organic phase was separated
  6. dry with materialdried over Na2SO4
  7. customthe solvent was removed by evaporation at reduced pressure
  8. customThe product thus obtained

出典と根拠

ORDレコード
ord-525bf8cd7c3841279ff6436a7852bb2b
出典データセット
uspto-grants-2013_04
特許番号
US08415476B2

反応ノート

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